超高效液相色谱-串联质谱法检测蜂蜜中的 甲硝唑含量

Determination of residues of metronidazole in honey by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  蜂蜜  甲硝唑

英文关键词:ultra performance liquid chromatography-tandem mass spectrometric  honey  metronidazole

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography- tandem mass spectrometry, UPLC-MS/MS)检测蜂蜜中的甲硝唑含量。方法 取混合均匀的蜂蜜样品加入饱和氯化钠溶液混合, 再经乙酸乙酯提取, 经阳离子交换小柱净化。采用UPLC-MS/MS技术, 以多反应监测模式检测, 以外标法定量。结果 甲硝唑在1~10.0 μg/L浓度范围内线性关系良好, 相关系数大于0.999, 回收率为76%, 检出限为0. 1 μg/kg, 相对标准偏差为3.4% (n=6)。结论 该方法快速、准确、灵敏, 可用于蜂蜜中甲硝唑的检测。

英文摘要:

      Objective To establish a method for the determination of metronidazole in honey samples by ultra performance liquid chromatography-tandem mass spectrometric (UPLC–MS/MS). Methods Honey samples were mixed with saturated sodium chloride and extracted with ethyl acetate, and then purified by cation exchange column. The metronidazole residues in the extracts were detected using UPLC–MS/MS (ESI+) with multiple reactions monitoring (MRM), and quantitated with external standard method. Results Metronidazole had a good linear relationship in the range of 1~10.0 μg/L with the linear correlation coefficient larger than 0.999. The recovery was 76%, the limits of detection (LOD) was 0.1 μg/kg, and the relative standard deviation (RSD) was 3.4% (n=6). Conclusion The proposed method is fast, accurate and sensitive, which is suitable for the determination of metronidazole residues in honey samples.